全文获取类型
收费全文 | 1787篇 |
免费 | 155篇 |
国内免费 | 100篇 |
专业分类
化学 | 1360篇 |
晶体学 | 17篇 |
力学 | 58篇 |
综合类 | 3篇 |
数学 | 74篇 |
物理学 | 530篇 |
出版年
2024年 | 4篇 |
2023年 | 9篇 |
2022年 | 13篇 |
2021年 | 42篇 |
2020年 | 64篇 |
2019年 | 31篇 |
2018年 | 46篇 |
2017年 | 59篇 |
2016年 | 87篇 |
2015年 | 68篇 |
2014年 | 84篇 |
2013年 | 162篇 |
2012年 | 83篇 |
2011年 | 125篇 |
2010年 | 109篇 |
2009年 | 139篇 |
2008年 | 116篇 |
2007年 | 101篇 |
2006年 | 123篇 |
2005年 | 103篇 |
2004年 | 112篇 |
2003年 | 69篇 |
2002年 | 51篇 |
2001年 | 38篇 |
2000年 | 27篇 |
1999年 | 24篇 |
1998年 | 28篇 |
1997年 | 27篇 |
1996年 | 20篇 |
1995年 | 15篇 |
1994年 | 18篇 |
1993年 | 9篇 |
1992年 | 11篇 |
1991年 | 2篇 |
1990年 | 3篇 |
1989年 | 2篇 |
1988年 | 3篇 |
1987年 | 5篇 |
1986年 | 2篇 |
1985年 | 2篇 |
1982年 | 2篇 |
1981年 | 3篇 |
1972年 | 1篇 |
排序方式: 共有2042条查询结果,搜索用时 15 毫秒
51.
52.
Lim LW Hirose K Tatsumi S Uzu H Mizukami M Takeuchi T 《Journal of chromatography. A》2004,1033(2):205-212
An on-line sample enrichment system was designed using monolithic precolumns in microcolumn LC. The monolithic ODS capillary columns were prepared via in situ sol-gel processes. The enrichment efficiency of the monolithic columns was tested by using phthalates as the analytes. The relative standard deviations (n = 6) for the retention time, peak area and peak height were between 0.4 and 1.2%, 0.9 and 5.5% and 0.4 and 3.9%, respectively. The system was linear (R2 > 0.99) within the working sample concentration and sample volume ranges. Comparing to 0.2 microl injection with a typical sample injector, the theoretical plate number of a same separation column was increased by 3-6-fold when the precolumn unit was used for sample injection. The recoveries of the analytes were between 88 and 120%, and the sample volume that could be injected into the system was increased up to 5000-fold. The limits of detection were improved by more than 2000-fold and were between 0.21 and 0.87 ng ml(-1) even with a UV absorbance detector. This system was applied to the determination of phthalates contained in laboratory distilled water and tap water samples. 相似文献
53.
Effect of Hydration–Dehydration Processes on the Structure and Porosity of Detemplated Silica Fibers
Kovalenko V. V. Tel'biz G. M. Bobonich F. M. 《Theoretical and Experimental Chemistry》2004,40(1):64-68
A study was carried out on the conditions of template removal (calcination or extraction by solvents) and hydration–dehydration processes on the hexagonal structure and porosity of detemplated fibers. The hydration–dehydration cycle leads to a decrease in fiber porosity, especially in fiber detemplation by extraction with surfactant solvents such as ethanol and acetic acid. 相似文献
54.
High Performance Liquid Chromatographic Analysis of Pharmaceuticals Using Oil-In-Water Microemulsion Eluent and Monolithic Column 总被引:1,自引:0,他引:1
Novel and efficient separations of pharmaceutical substances were achieved using oil-in-water microemulsion eluent and a conventional
C18 packing with a flow rate of 1 mL/min−1. Attempts to decrease analysis time was limited due to the high viscosity of the microemulsion which generated relatively
high back-pressures. Monolithic columns gave 3-fold lower back-pressures and allowed flow rates of 4 mL/min−1. with the same microemulsion mobile phase which permitted rapid separations to be achieved. Separation of a test-mix of paraben
preservatives was achieved in both isocratic and gradient mode in less than 1 min. The monolith-microemulsion combination
was applied to rapidly quantitatively analyse two formulated products with excellent linearity, accuracy and repeatability.
Quantitative analysis times were under 90 seconds. Successful quantitation of both nicotine lozenges and naprosyn tablets
was performed using this approach. 相似文献
55.
四羧基金属酞菁负载纤维素纤维的制备及其消臭性能研究 总被引:2,自引:0,他引:2
合成了四羧基铁酞菁(Fe-CPc)和四羧基钴酞菁(Co-CPc),并对其进行了元素分析和红外光谱表征.在酸性条件下,将四羧基金属酞菁负载到改性纤维素纤维上,制备得到消臭纤维.实验结果表明,在室温条件下,四羧基铁酞菁消臭纤维(FePcF)、四羧基钴酞菁消臭纤维(CoPcF)和混合金属酞菁消臭纤维(CoFePcF)3种功能性纤维都能有效去除甲硫醇、硫化氢、氨气和三甲胺,甲硫醇和硫化氢按催化氧化机理除去,而氨气和三甲胺按酸碱中和机理除去;3种消臭纤维对甲硫醇和硫化氢的消臭效果为CoFePcF>CoPcF>FePcF. 相似文献
56.
Hui-Juan Zhang 《Analytica chimica acta》2006,565(2):129-135
In this study, a polymer monolith microextraction (PMME) using a poly (methacrylic acid-ethylene glycol dimethacrylate) (MAA-EGDMA) monolith in conjunction with high-performance liquid chromatography (HPLC) was developed for the determination of 2,4-dinitrophenylhydrazine (DNPH) derivatives of several aldehydes in human saliva. The conditions for the labeling reactions of aldehydes with DNPH and followed extraction of the derivatives were optimized. The precision, recovery and detection limits were evaluated with spiked saliva. The limits of detection ranged from 0.43 to 1.40 μg/L. The inter-and intra-day relative standard deviations were less than 10%. The proposed method was successfully applied to the determination of aldehydes in saliva samples from a non-smoker, a passive smoker and a heavy smoker. 相似文献
57.
Xiong Wen Ye Yu Ping Zhang Ling Bo Qu Li Qun Fan Bo Li 《中国化学快报》2007,18(11):1399-1402
Microwave irradiation was firstly attempted for the preparation of organic-based monoliths of poly(styrene-divinylbenzene- methacrylic acid), which single step in situ polymerization was carried out during 15 min. The colunm permeability, electrophoretic and chromatographac behaviors were comparatively evaluated using pressure-assisted CEC, GEC and low pressure-driven separation modes. The largest theoretical plates for the preparing column could be close to 18,0000 plates/m for thiourea in the mode of p-CEC. It provided a viable alternative to traditional initiation means for the perparation of monolithic capillary columns. 相似文献
58.
Comparison between adsorption isotherm determination techniques and overloaded band profiles on four batches of monolithic columns 总被引:1,自引:0,他引:1
The adsorption isotherms of 4-tert.-butyl phenol were measured on four different monolithic columns, using three different techniques, classical frontal analysis (FA), the perturbation on a plateau method (PP) and the recently introduced numerical procedure known as the inverse numerical method (IN). This last approach requires only the recording of a few overloaded profiles and has the potential advantage of affording a dramatic decrease of the amounts of compounds, solvent, and time needed to determine accurate estimates of the coefficients of the isotherm. The reproducibility of the adsorption data measured on the four columns is discussed with reference to the specific techniques used for obtaining these data and to the most suitable equation used for modeling them. The data obtained for the different columns were highly consistent. The inverse numerical approach was confirmed to provide a powerful, accurate, and economic method for measuring single component adsorption data. 相似文献
59.
K. Chang Song 《Journal of Sol-Gel Science and Technology》1998,13(1-3):1017-1021
Mullite fibers were synthesized from an aqueous solution of aluminum isopropoxide, aluminum nitrate and tetraethylorthosilicate by the Sol-Gel method. The starting solution was prepared by adding aluminum isopropoxide and tetraethylorthosilicate simultaneously to an aluminum nitrate aqueous solution. The spinnability of the starting solution was investigated by varying the molar ratio of aluminum isopropoxide/aluminum nitrate in the solution. Gel fibers were obtained from solutions in a composition range of aluminum isopropoxide/aluminum nitrate of 3 to 5. Gels obtained from spinnable solutions appeared to have high homogeneity in the mixing of the Al/Si components, leading to a sharp 980°C exothermic peak in the DTA curve and a mullitization temperature of 1000°C. However, in the case of gels obtained from unspinnable solutions, a small 980°C exothermic peak was detected, and the mullitization temperature was as high as 1200°C, probably due to greater heterogeneity in the mixing of the Al/Si components. 相似文献
60.
Frank?WendlerEmail author Gerhard?Grane? Thomas?Heinze 《Cellulose (London, England)》2005,12(4):411-422
The thermal stability of cellulose/N-methylmorpholine-N-oxide (NMMO) solutions were investigated using UV/VIS spectrometry with a temperature programming cuvette and caloric measurements
by means of the Systag calorimeter RADEX (mini-autoclave). Both analytical methods allow to characterize the influences of
stabilizers and additives. With the temporal course of the optical density, temperature and pressure thermal runaway reactions
with gas evolution and accumulation of chromophoric degradation products were recognized. Kinetic model calculations compared
with UV/VIS measurements demonstrate the existence of autocatalytic reactions in cellulose/NMMO solutions. Varying the heating
rate autocatalysis can be proved by dynamic caloric measurements as well. 相似文献